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GB 1886.344-2021: National food safety standard - Food additives - DL-Alanine
GB 1886.344-2021
GB
NATIONAL STANDARD OF THE
PEOPLE?€?S REPUBLIC OF CHINA
National Food Safety Standard -
Food Additives - DL-Alanine
??????????????? DL-?????????
ISSUED ON: FEBRUARY 22, 2021
IMPLEMENTED ON: AUGUST 22, 2021
Issued by: National Health Commission of the People?€?s Republic of China;
State Administration for Market Regulation.
Table of Contents
1 Scope ... 3??
2 Chemical Name, Molecular Formula, Structural Formula and Relative
Molecular Mass ... 3??
3 Technical Requirements ... 3??
Appendix A Inspection Method ... 5??
Appendix B Reference Infrared Spectrogram of DL-alanine Standard
Substance ... 13??
National Food Safety Standard -
Food Additives - DL-Alanine
1 Scope
This Standard is applicable to the food additive DL-alanine, which is obtained through
enzymatic racemization, extraction and refining with L-alanine as the raw material.
2 Chemical Name, Molecular Formula, Structural
Formula and Relative Molecular Mass
2.1 Chemical Name
D-2-alanine, L-2-alanine
2.2 Molecular Formula
C3H7NO2
2.3 Structural Formula
2.4 Relative Molecular Mass
89.09 (in accordance with the international relative atomic mass of 2018)
3 Technical Requirements
3.1 Sensory Requirements
The sensory requirements shall comply with the requirements of Table 1.
Table 1 -- Sensory Requirements
D-alanine L-alanine
Appendix A
Inspection Method
A.1 General Rules
When other requirements are not specified, the reagents and water used in this
Standard refer to analytically pure reagents and Grade-3 water specified in GB/T 6682.
When other requirements are not specified, the standard solutions used in tests, and
standard solutions, preparations and products used for impurity determination shall be
prepared in accordance with the stipulations of GB/T 601, GB/T 602 and GB/T 603.
When it is not specified which solvent is used for preparation, the solutions used in
tests refer to aqueous solutions.
A.2 Identification Test
A.2.1 Reagent and material
Ninhydrin solution: weigh-take 0.1 g of ninhydrin; use water to dissolve it and dilute to
a constant volume of 100 mL.
A.2.2 Ninhydrin test
Weigh-take about 0.1 g of specimen, accurate to 0.01 g; dissolve it in 100 mL of water.
Take 5 mL of this solution; add 2 mL of ninhydrin solution. Heat it up to boiling; after a
certain time, it shall turn purple.
A.2.3 Infrared spectroscopy test
Adopt the potassium bromide smear method, in accordance with GB/T 6040,
determine the infrared absorption spectrum. The obtained infrared spectrogram shall
be consistent with the spectrogram of DL-alanine standard substance (see Appendix
B).
A.3 Determination of DL-alanine Content (calculated by dry basis)
A.3.1 Method summary
The specimen takes anhydrous formic acid as the auxiliary solvent, glacial acetic acid
as the solvent and crystal violet as the indicator. Use perchloric acid standard titration
solution to titrate it. In accordance with the volume of the consumed standard titration
solution of perchloric acid, calculate the content of DL-alanine.
A.3.2 Reagents and materials
A.3.2.1 Anhydrous formic acid.
When titrating the specimen, if the difference between the temperature of the standard
titration solution of perchloric acid and the temperature at the time of calibration
exceeds 10 ??C, then, it shall be re-calibrated; if it does not exceed 10 ??C, then, in
accordance with Formula (A.2), correct the concentration c of the standard titration
solution of perchloric acid, expressed in (mol/L).
Where,
c0---the concentration of the standard titration solution of perchloric acid at the time of
calibration, expressed in (mol/L);
0.0011---the expansion coefficient of glacial acetic acid;
T---the actual temperature of the standard titration solution of perchloric acid when
titrating the specimen, expressed in (??C);
T0---the temperature of the standard titration solution of perchloric acid at the time of
calibration, expressed in (??C).
The arithmetic mean value of parallel determination results shall prevail in the test
result. The absolute difference between two independent determination results
obtained under repeatability conditions shall not be greater than 0.3% of the arithmetic
mean value.
A.4 Determination of Loss on Drying
A.4.1 Instruments and equipment
A.4.1.1 Electrically heated drying oven.
A.4.1.2 Weighing bottle.
A.4.1.3 Desiccator.
A.4.2 Analytical procedures
Use a weighing bottle that has been dried to a constant mass to weigh-take 1 g ~ 2 g
of specimen, accurate to 0.0001 g. Place it in a 105 ??C ?? 2 ??C electrically heated drying
oven to dry for 3 h, then, take it out, cover it and put it into a desiccator. Cool it down
to room temperature (about 30 min), then, weigh it.
A.4.3 Result calculation
The mass fraction w2 of loss on drying in the specimen shall be calculated in
accordance with Formula (A.3).
The determination result shall be accurate to one decimal place. The arithmetic mean
value of parallel determination results shall prevail in the test result. The absolute
difference between two independent determination results obtained under repeatability
conditions shall not be greater than 0.05.
A.6 Determination of Transmittance
A.6.1 Instrument and equipment
Spectrophotometer.
A.6.2 Analytical procedures
Weigh-take 10 g of specimen, accurate to 0.01 g. Place it in a 100 mL beaker; add 70
mL of water to dissolve it. Transfer it into a 100 mL volumetric flask and dilute to the
scale; shake it well. Use a 1 cm cuvette, use water as the blank control; at the
wavelength of 430 nm, determine the light transmittance of the specimen solution;
record the reading.
The arithmetic mean value of parallel determination results shall prevail in the test
result. The absolute difference between two independent determination results
obtained under repeatability conditions shall not be greater than 0.2% of the arithmetic
mean value.
A.7 Determination of Specific Rotation
A.7.1 Reagent and material
Hydrochloric acid solution: 1 + 1.
A.7.2 Instrument and equipment
Polarimeter: equipped with sodium light (sodium spectrum D line 589.3 nm), with an
accuracy of ?? 0.01??.
A.7.3 Analytical procedures
Weigh-take 10 g of specimen that has been pre-dried at 105 ??C to a constant mass,
accurate to 0.0001 g. Place it in a 100 mL volumetric flask; add hydrochloric acid
solution to dissolve it and dilute to a constant volume; shake it well. Adjust the
temperature of the solution to 20 ??C. Use the above-mentioned specimen solution to
rinse the optical rotation tube for 3 times. Add the specimen solution (without bubbles)
into the optical rotation tube; observe and determine the optical rotation.
A.7.4 Result calculation
Specific rotation am (20 ??C, D), expressed in (??) ??? dm2 ??? kg-1, shall be calculated in
accordance with Formula (A.4).
A.8.4 Result determination
The turbidity of the specimen solution is shallower than that of the control solution, i.e.,
the chloride content is less than or equal to 0.02%.
A.9 Determination of Burning Residue
A.9.1 Reagents and materials
A.9.1.1 Concentrated sulfuric acid.
A.9.1.2 Sulfuric acid solution: 1 + 8.
A.9.2 Instruments and equipment
A.9.2.1 Platinum (or porcelain) crucible.
A.9.2.2 High-temperature furnace.
A.9.2.3 Desiccator.
A.9.3 Analytical procedures
Weigh-take about 2 g of specimen, accurate to 0.0001 g. Place it in a crucible that has
been burnt at 800 ??C ?? 25 ??C to a constant mass. Slowly dropwise add 1 mL of sulfuric
acid solution to completely moisten the specimen. Firstly, heat it up on an electric
furnace with a small fire, until the specimen has just begun to be carbonized, then,
remove it and cool it down. Then, dropwise add 0.5 mL of concentrated sulfuric acid;
use the above-mentioned method to heat it up, until the sulfuric acid vapor is exhausted;
transfer it into a high-temperature furnace at 800 ??C ?? 25 ??C and burn it for 45 min.
When the temperature of the furnace drops to 200 ??C, remove the cover, put it in the
desiccator to cool down for 30 min, then, weigh it.
A.9.4 Result calculation
The mass fraction w3 of burning residue in the specimen shall be calculated in
accordance with Formula (A.5).
Where,
m5---after burning, the mass of the crucible and the specimen, expressed in (g);
m3---the mass of the crucible, expressed in (g);
m4---the mass of the crucible and the specimen, expressed in (g).